4-Methylamino antipyrine determination in human plasma by high-performance liquid chromatography tandem mass spectrometry |
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| Authors: | Aleksandra Nikitina Geliia Gildeeva Alexander Grigoriev Alla Sidorova |
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| Affiliation: | 1. Bioanalytical Laboratory CSU “Analytical Spectrometry”, St Petersburg, Russia;2. Department of organization and managment of the circulation of medicines, I.M.Sechenov Fist Moscow State Medical University, Moscow, Russia;3. Bioanalytical Laboratory CSU “Analytical Spectrometry”, St Petersburg, Russia Center of Shared Usage “The analytical center of nano- and biotechnologies of SPbPU”, Peter the Great St Petersburg Polytechnic University, St Petersburg, Russia |
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| Abstract: | In the present study, a simple and rapid method for metamizole metabolite 4-methylamino antipyrine (MAA) determination in human plasma was developed, validated and successfully applied to a clinical trial. Chromatographic separation was achieved in HILIC mode on a YMC-Pack SIL column (100 × 2.0 mm; S-5 μm, 30 nm), with a mobile phase consisting of acetonitrile, water and formic acid. Protein precipitation of a small plasma volume using acetonitrile was selected for sample preparation. The multiple reaction monitoring transitions in the positive ionization mode were m/z 218.2 → 56.2 for MAA and m/z 221.2 → 56.2 for MAA-d3 (IS, internal standard). Concentration levels of MAA calibration standards were in the range of 0.100–20 μg/ml. Metamizole conversion into MAA in both water and organic media was investigated, and the level of the conversion in commercially available injection solutions was estimated. |
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| Keywords: | 4-methylamino antipyrine HPLC–MS/MS human plasma hydrolyzation-oxidation reaction metamizole |
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